CN103215632B - A kind of growth method of large size c orientation sapphire single-crystal - Google Patents
A kind of growth method of large size c orientation sapphire single-crystal Download PDFInfo
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- CN103215632B CN103215632B CN201310113549.7A CN201310113549A CN103215632B CN 103215632 B CN103215632 B CN 103215632B CN 201310113549 A CN201310113549 A CN 201310113549A CN 103215632 B CN103215632 B CN 103215632B
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Abstract
The invention discloses a kind of growth method of large size c orientation sapphire single-crystal, comprise placement seed crystal, feed, vacuumize, start the steps such as helium, heating material, crystal growth, cooling annealing, detection and process; The diameter 260mm crucible used at present is increased to diameter 285mm crucible by the present invention, and without the need to changing former thermal field, be optimized long brilliant parameter, charging capacity is increased to 60kg from 37kg, thus improves production efficiency, reduces cost.
Description
Technical field
The invention belongs to sapphire technical field, relate to a kind of growth method of c orientation sapphire single-crystal, the crucible particularly relating to a kind of large-sized use diameter 285mm carries out the method for c orientation Sapphire Crystal Growth.
Background technology
Sapphire (Sapphire) is a kind of aluminum oxide (α-Al
2o
3) monocrystalline, be also called corundum, crystal has excellent optical property, mechanical property and chemical stability, intensity is high, hardness is large, resistance to erosion, can work under the mal-condition close to 2000 DEG C of high temperature, thus be widely used in the window material of infrared military installation, satellite spatial technology, high intensity laser beam.The crystalline network of its uniqueness, excellent mechanical property, good thermal property make sapphire crystal become the semi-conductor GaN/Al of practical application
2o
3photodiode (LED), the substrate material that large-scale integrated circuit SOI and SOS and superconducting nano structural membrane etc. are ideal.In recent years, along with the development of modern science and technology, new requirement is constantly proposed to the size of sapphire crystal material, quality.Such as, the American National Natural Science Fund In The Light council is as the sapphire crystal of LIGO (LaserInterferometerGravitationalWaveObservatory) beam splitting lens in the works, crystalline size: ￠ 350 × 120mm, optical homogeneity: △ n<2 × 10
-7, weak absorption coefficient (1064nm): 10
-6/ cm; The window material of infrared imaging detection equipment, lowest calibre is ￠ 150mm, service band transmitance >80%.Particularly high-brightness white-light LED is as general illumination device of future generation, has the advantages such as green energy conservation.Sapphire Substrate is the main substrate of gallium nitrate based white light LEDs, and the demand in market is huge.
Utilized oxyhydrogen flame to melt natural ruby powder and potassium bichromate from 1885 by Fremy, Feil and Wyse and made sensational " Geneva ruby " at that time, the sapphire research of Artificial Growth so far has the history of more than 100 year.During this period, in order to adapt to the development of science and technology and industrial production for the particular requirement of sapphire crystal quality, size, shape, in order to improve yield rate, the utilization ratio of sapphire crystal and reduce costs, carried out large quantifier elimination to sapphire growth method and correlation theory thereof, achievement is remarkable.So far had higher state of the art and larger throughput, the crystal growth equipment single crystal growing furnace of adequate and systematic service for it also obtains development at full speed thereupon.Along with the sharply expansion of sapphire crystal application market, its equipment and technology also achieve in last century end and develop rapidly, and crystalline size expands current 12 inches to from 2 inches.
Low cost, in high quality growing large-size sapphire single-crystal have become the current urgent task faced.All things considered, sapphire crystal growth mode can be divided into solution growth, melt growth, vapor phase growth three kinds, wherein melt growth mode is fast because having growth velocity, the features such as the high and perfection of crystal of purity is good, and become the most frequently used crystal growth pattern preparing large size and specified shape crystal.Can be used at present mainly contain flame melt method, crystal pulling method, zone melting method, EFG technique, crucible Mobile Method, heat-exchanging method, temperature gradient method, kyropoulos etc. with the method for melt growth mode Artificial Growth sapphire crystal.
My company uses diameter 260mm crucible to carry out c orientation sapphire crystal growth at present, and charging capacity, at about 37kg, because charging capacity is little, cannot realize increasing production capacity and there is the problems such as tooling cost is higher.
Therefore, for above-mentioned technical problem, be necessary to provide a kind of larger sized crucible to carry out the growth of the sapphire single-crystal of c orientation, to overcome above-mentioned defect.
Summary of the invention
In view of this, the object of the present invention is to provide the crucible of a kind of large-sized use diameter 285mm to carry out the method for c orientation Sapphire Crystal Growth, thus increase charging capacity, enhance productivity, reduce costs.
For achieving the above object, the invention provides following technical scheme:
The growth method of large size c orientation sapphire single-crystal of the present invention, specifically comprises the steps:
(1) seed crystal is placed: be placed in the seed slot of diameter 285mm crucible by c orientation seed crystal;
(2) feed: high purity aluminium oxide raw material is put into crucible, close bell, start cooling water recirculation system;
(3) vacuumize: start vacuum system, furnace chamber pressure is evacuated to below 0.015Torr;
(4) helium is started: start helium cooling system, adjustment helium gas flow is 40 ~ 100slm, prevents seed crystal in material process from melting completely;
(5) material is heated: start heating system and heat up, power is increased with 3.33KW/h, after rising to 11.55KW, 61KW is risen to 11.55KW/h, heat up with 3 DEG C/h, when detecting thawing position and reaching 120mm above target value, heat up with 1.25 DEG C/h, until high purity aluminium oxide starts fusing, control seed portion is melted;
(6) crystal growth: first lower the temperature with 1 DEG C/h, helium gas flow increase per hour 1slm, be respectively 0.3 DEG C/h and 0.12 DEG C/h with rate of temperature fall again to lower the temperature, every 12h detects, and calculates crystal growth rate, if growth velocity is more than 1.8mm/h, rate of temperature fall is reduced according to actual measurement numerical value, until when continuous probe 3 probe locations are identical, confirm that crystal completes growth, then carry out the cooling of 24h;
(7) cooling annealing: bushing position rises with 2mm/h, reduce power and be reduced to 30KW, 8KW, 2KW respectively until 0KW with 0.6KW/h, 0.3KW/h, 0.2KW/h, 0.2KW/h, when annealing stage starts, and be filled with argon gas with 20slm, until reach 500Torr, cool and unload after 24 hours;
(8) detect and process: crystal ingot detects to coming out of the stove, and whether has crystal boundary, bubble, cracking, then excises end to end, drawing and carry out drawing rod.
Preferably, the well heater that described heating adopts is birdcage shape, netted tubular tungsten well heater or tubular graphite heater.
Preferably, described crucible is tungsten crucible, molybdenum crucible, miramint crucible or iridium crucible, described crucible bottom form be in right angle, fillet or chamfering form.
Preferably, described high purity aluminium oxide raw material is Al
2o
3powder, Al
2o
3biscuit, granular Al
2o
3and any one or the two or more combinations in sapphire broken grain.
The diameter 260mm crucible used at present is increased to diameter 285mm crucible by the present invention, and without the need to changing former thermal field, be optimized long brilliant parameter, charging capacity is increased to 60kg from 37kg, thus improves production efficiency, reduces cost.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme in the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing for the present invention in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the structural representation of diameter 260mm crucible used in prior art;
Fig. 2 is the structural representation of the present invention's diameter 285mm crucible used.
Embodiment
Be described in further detail below in conjunction with the growth method of embodiment to the large size c orientation sapphire single-crystal of invention.
1, long brilliant stove prepares
Check thermal field, note abnormal phenomenon, especially thermal field bend, loss, variable color or fragmentation part.The fragment of thermal field in cleaning stove.Check the position of crucible and GCD and determine that they are in correct position.Check the service condition of probe, if there is conditions, three stoves used by replacing probe: A, probe; B, probe bend, break or can not with insulation probe aperture centering; C, probe there is excessive settling or become very crisp.
Centering is carried out to pyrometer hole.With IPA and dust-free paper thoroughly clear up inside and outside crucible, the top of crucible pole groove, crucible pole, then one deck parting agent is smeared to crucible pole groove and crucible pole top.Could install after parting agent will solidify 30 ~ 60 minutes, with vacuum clamp, crucible is arranged in stove.In crucible groove, put into model seed crystal, decline probe, see whether centering measure seeding target value.Confirm whether initial helium gas flow is 70SLPM.
2, raw material loads
Crucible and GCD position are placed on respectively the position of 50 and 20, the seed crystal checked is put into seed slot, rotate the center be confirmed to be at seed slot.By A in the face of pyrometer direction.One piece of larger sapphire raw material block is vertically put into above seed crystal, pushes down seed crystal, prevent seed crystal from tilting.Then around seed crystal, pile one deck powder, then replace stacking until raw material all installs with block material and powder.Then decline probe measurement raw material height and crucible cover height, and centering is carried out to crucible cap bore.After completing, probe location is risen in the middle of raw material and crucible cover, cover bell, start.
3, find time and hunt leak
Vacuum is evacuated to below 0.015Torr, hunts leak, and leakage rate is at below 0.015Torr.
4, melt
Carry out heating material, the H1 stage, power is increased with 3.33KW per hour, rise to soak2 hour after 11.55KW, enter the H2 stage, rise to soak2 hour after 61KW with 11.55KW per hour, system enters Melt1, after this program has been run, current PYROMETER numerical value is calculated numerical value according to recipe formula and inputs in Melt2TEMPERATUREEND, enter the Melt2 stage.System enters the MELT3 stage, with 3 degrees Celsius of/hour intensifications, opens " TRENDSCREENS " interface, if POWERBOW occurs, within 2 hours, starts detection later melt position at it.In Melt3 process, when detecting thawing position and reaching 120mm above target value (target value+120mm), manually by the final temperature of current PYROMETER temperature value input Melt3 (i.e. Melt4 starting temperature), enter Melt4 to run, heat up with 1.25 degrees Celsius/hour, per hourly to detect, until reach target value.
5, the long brilliant stage (the long brilliant stage is temp-controled mode)
In the GROWTH1 stage, with 1 degree Celsius of/hour cooling, helium gas flow increased with 1slm/ hour, and this stage is without the need to detecting probe position.
When long brilliant process proceeds to " Growth2-3 " stage, rate of temperature fall is respectively 0.3 degree Celsius/hour and 0.12 degree Celsius/hour, within every 12 hours, detects, and calculates crystal growth rate, if growth velocity is more than 1.8mm/ hour, rate of temperature fall is reduced according to actual measurement numerical value.Until when continuous probe 3 probe locations are identical, confirm that crystal completes growth, then carry out the cooling of 24 hours, enter next stage.
6, annealing stage (annealing stage is power control mode)
Bushing position rose to 125 positions with 2mm/ hour by 50, reduce power with 0.6KW/ hour, 0.3KW/ hour, 0.2KW/ hour, 0.2KW/ hour be reduced to 30KW, 8KW, 2KW respectively until 0KW, when annealing stage starts, and be filled with argon gas with 20slm, until reach 500Torr, cool and unload after 24 hours.
7, detect and process
To coming out of the stove, crystal ingot detects, and whether has crystal boundary, bubble, cracking, then excises end to end, draws and carries out drawing rod.
In sum, the diameter 260mm crucible used at present is increased to diameter 285mm crucible by the present invention, and without the need to changing former thermal field, be optimized long brilliant parameter, charging capacity is increased to 60kg from 37kg, thus improves production efficiency, reduces cost.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.Any Reference numeral in claim should be considered as the claim involved by limiting.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (4)
1. a growth method for large size c orientation sapphire single-crystal, is characterized in that, comprises the steps:
(1) seed crystal is placed: be placed in the seed slot of diameter 285mm crucible by c orientation seed crystal;
(2) feed: high purity aluminium oxide raw material is put into crucible, close bell, start cooling water recirculation system;
(3) vacuumize: start vacuum system, furnace chamber pressure is evacuated to below 0.015Torr;
(4) helium is started: start helium cooling system, adjustment helium gas flow is 40 ~ 100slm, prevents seed crystal in material process from melting completely;
(5) material is heated: start heating system and heat up, power is increased with 3.33KW/h, after rising to 11.55KW, 61KW is risen to 11.55KW/h, heat up with 3 DEG C/h, when detecting thawing position and reaching 120mm above target value, heat up with 1.25 DEG C/h, until high purity aluminium oxide starts fusing, control seed portion is melted;
(6) crystal growth: first lower the temperature with 1 DEG C/h, helium gas flow increase per hour 1slm, be respectively 0.3 DEG C/h and 0.12 DEG C/h with rate of temperature fall again to lower the temperature, every 12h detects, and calculates crystal growth rate, if growth velocity is more than 1.8mm/h, rate of temperature fall is reduced according to actual measurement numerical value, until when continuous probe 3 probe locations are identical, confirm that crystal completes growth, then carry out the cooling of 24h;
(7) cooling annealing: bushing position rises with 2mm/h, reduce power and be reduced to 30KW, 8KW, 2KW respectively until 0KW with 0.6KW/h, 0.3KW/h, 0.2KW/h, 0.2KW/h, when annealing stage starts, and be filled with argon gas with 20slm, until reach 500Torr, cool and unload after 24 hours;
(8) detect and process: crystal ingot detects to coming out of the stove, and whether has crystal boundary, bubble, cracking, then excises end to end, drawing and carry out drawing rod.
2. growth method according to claim 1, is characterized in that: the well heater that described heating adopts is birdcage shape, netted tubular tungsten well heater or tubular graphite heater.
3. growth method according to claim 1, is characterized in that: described crucible is tungsten crucible, molybdenum crucible, miramint crucible or iridium crucible, described crucible bottom form be in right angle, fillet or chamfering form.
4. growth method according to claim 1, is characterized in that: described high purity aluminium oxide raw material is Al
2o
3powder, Al
2o
3biscuit, granular Al
2o
3and any one or the two or more combinations in sapphire broken grain.
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|---|---|---|---|---|
| CN103726105A (en) * | 2013-10-11 | 2014-04-16 | 中国科学院上海光学精密机械研究所 | Growing apparatus and method for Ti sapphire crystal |
| CN104152984B (en) * | 2014-08-12 | 2017-03-15 | 杭州铸泰科技有限公司 | A kind of reusable crucible for oriented growth sapphire single-crystal |
| CN104975341A (en) * | 2015-06-24 | 2015-10-14 | 吴倩颖 | Method for increasing batch feeding amount for single crystal pulling |
| CN105088331B (en) * | 2015-08-26 | 2017-10-13 | 哈尔滨工业大学 | A kind of C is to growing sapphire monocrystalline with small angle crucible |
| CN105525355B (en) * | 2015-11-06 | 2018-05-08 | 浙江露通机电有限公司 | Large size sapphire crystal in-situ annealing technique |
| CN105369345B (en) * | 2015-12-03 | 2018-01-26 | 河南西格马晶体科技有限公司 | A kind of crucible and preparation method for being used to prepare sapphire monocrystal |
| CN105648520A (en) * | 2016-03-18 | 2016-06-08 | 江苏中电振华晶体技术有限公司 | Seed crystal capable of reinforcing seeding temperature signals and seeding method thereof |
| CN107130289A (en) * | 2017-06-13 | 2017-09-05 | 江苏吉星新材料有限公司 | A kind of growing method for improving heat exchange large size sapphire crystal |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5277366A (en) * | 1992-07-09 | 1994-01-11 | Ursic Thomas A | High pressure fluid jet orifice made of oxygen enhanced sapphire and process for making same |
| CN101323978A (en) * | 2008-07-29 | 2008-12-17 | 成都东骏激光有限责任公司 | Large size sapphire crystal preparing technology and growing apparatus thereof |
| CN101580963A (en) * | 2009-06-26 | 2009-11-18 | 哈尔滨工大奥瑞德光电技术有限公司 | SAPMAC method for preparing sapphire single-crystal with size above 300mm |
| CN201411510Y (en) * | 2009-06-26 | 2010-02-24 | 哈尔滨工大奥瑞德光电技术有限公司 | Birdcage-structured resistance heating element of single crystal furnace for growth of big size sapphire |
| CN101962800A (en) * | 2010-10-09 | 2011-02-02 | 王楚雯 | Device for producing single crystal ingot by directional solidification method |
| CN101962798A (en) * | 2009-07-22 | 2011-02-02 | 国立大学法人信州大学 | Be used to produce the method and apparatus of sapphire single-crystal |
| CN201817570U (en) * | 2010-10-09 | 2011-05-04 | 王楚雯 | Device for manufacturing single crystal ingots through directional solidification method |
| CN102140689A (en) * | 2011-03-08 | 2011-08-03 | 中国科学院上海硅酸盐研究所 | Method for growing sapphire crystal |
| CN102644113A (en) * | 2012-05-14 | 2012-08-22 | 苏州海铂晶体有限公司 | Production method and equipment of c-oriented sapphire single crystal |
| CN102732944A (en) * | 2011-04-02 | 2012-10-17 | 江苏同人电子有限公司 | Crystal growth technology and crystal growth furnace |
| CN102828232A (en) * | 2012-09-25 | 2012-12-19 | 倪屹 | Three-dimensional sapphire crystal growing device |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100101387A1 (en) * | 2008-10-24 | 2010-04-29 | Kedar Prasad Gupta | Crystal growing system and method thereof |
-
2013
- 2013-04-02 CN CN201310113549.7A patent/CN103215632B/en not_active Expired - Fee Related
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5277366A (en) * | 1992-07-09 | 1994-01-11 | Ursic Thomas A | High pressure fluid jet orifice made of oxygen enhanced sapphire and process for making same |
| CN101323978A (en) * | 2008-07-29 | 2008-12-17 | 成都东骏激光有限责任公司 | Large size sapphire crystal preparing technology and growing apparatus thereof |
| CN101580963A (en) * | 2009-06-26 | 2009-11-18 | 哈尔滨工大奥瑞德光电技术有限公司 | SAPMAC method for preparing sapphire single-crystal with size above 300mm |
| CN201411510Y (en) * | 2009-06-26 | 2010-02-24 | 哈尔滨工大奥瑞德光电技术有限公司 | Birdcage-structured resistance heating element of single crystal furnace for growth of big size sapphire |
| CN101962798A (en) * | 2009-07-22 | 2011-02-02 | 国立大学法人信州大学 | Be used to produce the method and apparatus of sapphire single-crystal |
| CN101962800A (en) * | 2010-10-09 | 2011-02-02 | 王楚雯 | Device for producing single crystal ingot by directional solidification method |
| CN201817570U (en) * | 2010-10-09 | 2011-05-04 | 王楚雯 | Device for manufacturing single crystal ingots through directional solidification method |
| CN102140689A (en) * | 2011-03-08 | 2011-08-03 | 中国科学院上海硅酸盐研究所 | Method for growing sapphire crystal |
| CN102732944A (en) * | 2011-04-02 | 2012-10-17 | 江苏同人电子有限公司 | Crystal growth technology and crystal growth furnace |
| CN102644113A (en) * | 2012-05-14 | 2012-08-22 | 苏州海铂晶体有限公司 | Production method and equipment of c-oriented sapphire single crystal |
| CN102828232A (en) * | 2012-09-25 | 2012-12-19 | 倪屹 | Three-dimensional sapphire crystal growing device |
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